• Volume 27,Issue 9,2010 Table of Contents
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    • >Surfactants
    • Study on the Microstructure of Formamide/ Tri(ethyleneglycol)monododecyl Ether /n-Octane by UV-Visible Spectroscopy

      2010, 27(9).

      Abstract (463) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:Oil-continuous microemulsion phase behavior formed by formamide (polar phase), n-octane (oil phase), tri(ethyleneglycol)monododecyl ether (AEO3) was investigated. Using the methyl orange (MO) and methylene blue (MB) as absorption probes, the microstructure of nonaqueous microemulsions was probed with UV-vis spectroscopy measurements as the absorption maximum is changed with the polarities of the pure solvents, micelles and reverse-micelles systems. The results indicated that an n-octane continuous structure with formamide nano-droplets formed in formamide/ AEO3 /n-octane system.

    • >Review and monographs
    • Research on Synthesis of Proton Pump Inhibitors

      2010, 27(9).

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      Abstract:Clinically duodenal and peptic ulceration are the most common diseases. Control of the gastric pH with antisecretory drugs has proven to be an effective method in the treatment of duodenal and peptic ulcers. Proton pump inhibitors have been proved to be the most effective drugs in curing ulcers. The research advance of various synthetic methods of proton pump inhibitors were reviewed. The research advance for the synthesis of key intermediates 2-mercapto-benzimidazoles,2-mercapto-imidazo[4,5-b]pyridines and 2-chloromethyl pyridine compounds were summarized. The optimum synthetic scheme was discussed.

    • >Functional materials
    • Study on functionalization and fluorescence properties of dendritic poly(amine-ester)

      2010, 27(9).

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      Abstract:Poly(amine-ester)-benzaldehyde dendrimer(PAE-BZA) was synthesized from ethyl enediamine (EDA), trimethylolpropane triacrylate (TMPTA) and benzaldehyde (BZA), the yield was 60.82%. The structure of PAE-BZA was characterized by IR、1H-NMR and 13C-NMR. The effects of different concentrations, different solvents and Sn2 on fluorescence properties of the dendrimer were studied. When acetone was solvent, fluorescence of 0.5mmol/L PAE-BZA was strongest. Take acetone, the methyl alcohol, DMSO, DMF and ethyl alcohol as solvent, fluorescence of PAE-BZA in ethyl alcohol was strongest. Fluorescence of PAE-BZA was first decreased then increased by Sn2 in the solution, and the complexing order of N atom was from periphery to internal.

    • Interactions between Sodium Tetrafluoroethylene Pentamer-oxylbenzenesulfonate and Octyltriethylammonium Bromide

      2010, 27(9).

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      Abstract:The surface tension of the mixtures of cationic-anionic hydrogenated-fluorinated surfactants composed of octyltriethylammonium bromide (C8H17N(CH2CH3)3Br, C8NE) and sodium tetrafluoroethylene pentamer-oxylbenzenesulfonate (C10F19OC6H4SO3Na, 6201) with different molar ratios was measured. The critical micelle concentration (cmc), the minimum surface tension (γcmc), total amount adsorbed, the composition of surface adsorbed layer at different surface tension values and the micelle composition at cmc calculated by Gibbs-Duhem equation were obtained. The molecular interaction parameter βm and the micelle composition after cmc were estimated by the regular solution theory. It showed that, the cmc of C8NE-6201 mixtures was significantly smaller than that of individual component, which was also consistent with the large negative value of βm and thus the strong molecular interactions in micelles. However, the γcmc of C8NE-6201 mixtures were changed very small compared with single 6201, which might be attributed to the long hydrophobic chain of 6201 and the solubility was decreased when C8NE coexisted. Because of its strong hydrophobicity, 6201 primarily comprised the surface adsorbed layer and the micelle that were initially formed, while oppositely-charged C8NE offered the effect of synergism. The micelle composition after cmc, x6201m (the molar fraction of 6201 in micelle), however, maintained approximately in the range 0.6~0.7, indicating that cationic-anionic electrostatic interaction was the major role in micelle formation after cmc.

    • Preparation and characterization of multiple acid-catalyzed carbon aerogels under ambient conditions

      2010, 27(9).

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      Abstract:A sol-gel polymerization has been employed to prepare organic aerogels through the reaction of resorcinol and formaldehyde with multiple organic acid as catalyst and cetyltrimethylammonium bromide as surfactant. The gels were dried under ambient pressure and carbonized at high temperature. The samples were characterized by methylene blue adsorption test, scanning electron microscopy (SEM), and X-ray diffraction analysis (XRD). The results indicated that the carbon aerogels are uniform spheres, and the microspheres were abundant in connected pore for the electronic transfering. The X-ray diffraction pattern showed two broad peaks, indicating that the materials are amorphous . The methylene blue adsorption test shows that there are a lot of mesoporous in the materiales and the surface area is as high as 740 m?g. Cyclic voltammetry (CV) was used to study the electrochemical performance of the materials . The test results show that the samples have perfect conductivity , high specific capacitance and stable performance with a longer cycle life. They could be used as the effective electrode materials for supercapacitors.

    • >Surfactants
    • Recycling of the starch glycoside from the upper liquid

      2010, 27(9).

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      Abstract:This paper studies the recycling of the starch glycoside that was synthesized by the glycoside exchange with starch and alcohol. The chemical structures of the product which was separated from the upper liquid, were characterized with primarily FT-IR, GC-MS and the physicochemical properties were analysed. The upper starch glycoside was contrasted with the lower starch polyglycosides. The results demonstrated that the product of the upper liquid is starch glycoside, surface tension is from 24.77~29.50 mN/m and the CMC is 2.0 ×10-3 g/L.

    • >Modernization technology of traditional Chinese medicines
    • Extracts from Ipomea pes-caprae (Linn.) Sweet in ASE and Study on Antioxidant Activity

      2010, 27(9).

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      Abstract:The Ipomea pes-caprae (Linn.) Sweet leaves extracts were extracted with different polar solvents by ASE. The antioxidant activity of different extracts were evaluated by DPPH assay. The antioxidant activity of ascorbic acid > ethyl acetate extract > ethanol extract > methanol extract > petroleum ether extracts, its IC50 values were 0.2034 mg/mL, 0.8362 mg / mL, 0.8688 mg/mL, 1.8675 mg/mL and 6.6283 mg/mL. The results showed the Ipomea pes-caprae (Linn.) Sweet leaves extracts had an antioxidant activity, and ethyl acetate extract was highest in all extracts.

    • >Catalysis,separation and purification technology
    • Study on Improving Reducing Sugar Yield of Steam-Explosive Corn Stalk by Enzymatic Hydrolysis

      2010, 27(9).

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      Abstract:Corn stalk was treated by steam explosion, and the structure of untreated/treated corn stalk were detected by Scanning Electron Microscope (SEM) and X-ray diffraction(XRD), while their chemical composition were also investigated. Comparing with the untreated corn stalk, reducing sugar yield of treated corn stalk was increased by 197% after hydrolyzing for 24h. The relative content of hemicelluloses and solvend decreased, while cellulose increased by 29.7%; the compact structure of corn stalk was remarkably destroyed. The optimum steam exploded process condition: operating pressure 2.2MPa, solid-liquid ratio 1:1, reaction time 9min and materials size 40-60 meshes.

    • Synthesis of methyl palmitate catalyzed by solid acid Zr(SO4)2/TiO2

      2010, 27(9).

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      Abstract:Biodiesel was synthesized by industrial palmitic acid and methanol, using solid acid Zr(SO4)2/TiO2 as catalyst. Effects of mass fraction of Zr (SO4)2 in the catalyst, calcination temperature and time of catalyst, mass ratio of methanol to industrial palmitic acid, catalyst dosage and reaction time on the esterification rate were investigated. The catalyst and ester product were analysed by GC-MS, FTIR and DTG/DTA methods. Assessment experiments show that the catalytic activity of the supported Zr(SO4)2/TiO2 catalyst was higher than the unsupported Zr(SO4)2 catalyst. The esterification rate can reach at 98.9% under the following conditions: calcination temperature of catalyst 400 ℃, loading amount of Zr(SO4)2(based on total mass of catalyst) 65%, mass ratio of methanol to industrial palmitic acid 12/25, mass fraction of Zr (SO4)2/SiO2 in palmitic acid 8.0% and reaction time 5 h. Analysis result of GC-MS showed that the ester product were mainly hexadecanoic acid methyl ester and 10-octadecenoic acid methyl ester.

    • >Perfumes and essences
    • Preparation and Characterization of Tuberose Fragrance-Loaded Chitosan Nanoparticles

      2010, 27(9).

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      Abstract:On the base of using sodium tripolyphosphate(TPP) as crosslinker, tuberose fragrance-loaded chitosan nanoparticles were prepared by ionic gelation method. The effects of the mass concentration of chitosan、the mass concentration of tuberose fragrance、the mass ratio between emulsifier and fragrance and the reaction time to the size distribution of tuberose fragrance-loaded chitosan nanoparticles were studied. The tuberose fragrance-loaded chitosan nanoparticles were characterized by dynamic light scattering(DLS)、transmission electron microscopy(TEM)、infrared spectroscopy(IR) and thermogravimetric analysis(TGA). Results showed that the average particle size was 138nm, the polydispersity was 0.100 and the fragrance loading capacity was 28.4% when the chitosan mass concentration was 1.71g/L、the fragrance mass concentration was 1.72g/L、m(emulsifier):m(fragrance)=1:2 and reaction time was 1h. Under high temperature, the release rate of tuberose fragrance loaded by chitosan nanoparticles was decreased.

    • >Drug and cosmetic materials
    • Ths Synthesis of Xylopinine

      2010, 27(9).

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      Abstract:3,4-Dimethoxyphenylacetonitrile was employed as the staring material to give 3,4-dimethoxyphenylethylamine and 3,4-dimethoxyphenylacetic acid via hydrolysis and hydrogenation reduction, respectively. The resulting two intermediates were reacted to produce the amide, which underwent Bischler-Napieralski cyclization, potassium borohydride reduction, and Pictet-Spengler reaction with formaldehyde to give racemic xylopinine in an overall yield of 47%.

    • Synthesis of cyclo(Leu-N-MeLeu-Leu-Leu- N-MeLeu)

      2010, 27(9).

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      Abstract:Cyclo(Leu-N-MeLeu-Leu-N-MeLeu-Leu), with antiproliferative activities, has been synthesized with leucine for the starting material. The efficiency of cyclization is 53.7%. The structures of product and intermediates were characterized by 1HNMR, 13CNMR and MS. All reactions were mild.

    • Synthesis of Ferrocenyl Thioacetyl Morpholine

      2010, 27(9).

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      Abstract:Acetylferrocene was synthesized via Friedel-Crafts acylation with ferrocene and acetyl chloride as raw material, dichloromethane as solvent, zinc oxide as catalyst. And optimal condition was concluded by orthogonal, its yield was 86% under the reaction conditions of molar ratio of ferrocene to acetyl chloride and zinc oxide 1:3:1.2. Ferrocenyl thioacetyl morpholine was synthesized via Willgerodt-Kinder reaction with acetylferrocene, sulfur and morpholine as starting material. The optimal condition was concluded by orthogonal, its yield was 65% under the reaction conditions of molar ratio of acetylferrocene to sulfur and Morpholine 1:3:6, reaction temperature was 128℃, reaction time was 4 hours.The product was characterized by elemental analysis, IR, 1HNMR.

    • >Rubber and plastics auxiliaries
    • Synthesis of 5,5-dimethyl-2-phospha-1,3-dioxan-2-yl acrylamide methoxy phosphate

      2010, 27(9).

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      Abstract:A novel intumescent flame retardant (IFR) 5,5-dimethyl-2-phospha-1,3-dioxan-2-yl acrylamide methoxy phosphate was synthesized with neopentyl glycol, phosphorus oxychloride and N-hydroxymethyl acrylamide, using triethylamine as acid acceptor and CuCl as catalyst. The structure of the compound was characterized by elemental analysis, FTIR and 1H NMR. The yield of the compound was 75.3% with the molar ratio of N-hydroxymethyl acrylamide to triethylamine being 1:1, the mass fraction of CuCl being 1.5% N-hydroxymethyl acrylamide, and the reaction in ice-water bath for 2 h at first and then in room temperature for10 h. And the thermal properties of the compound were tested by TG and DSC techniques. The TG curves of the compound indicates that the initial thermal decomposition temperature is about 210℃, and there is about 40% char residue left at 800℃, indicating that the title compound has a good thermal stability and a char forming capability.

    • Preparation of bis[ (triethoxsily)propyl]-disulfide in aqueous phase

      2010, 27(9).

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      Abstract:With γ-chloropropyltriethoxysilane (γ2),sulfur and sodium disulfide as the starting materials,the bis-(triethoxysilypropyl)disulfide (Si-75) was synthesized in aqueous phase by using phase transfer catalysis technique and adding buffer to the reaction system to control its pH value which can refrain the hydrolysis of γ2. In this paper, the mol ratio of sulfur with sodium disulfide, γ2 with sodium polysulfide and sodium carbonate with sodium disulfide, reaction temperature, the mass of phase transfer catalyst and some other conditions are all studied. Using this method, we got the sample with yield of 95.4%,sulfur content of 13.5% and flaxen appearance .

    • >Dyeing and finishing auxiliaries
    • Synthesis and Application of Side-chain Polyether-containing Aminopolysiloxane

      2010, 27(9).

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      Abstract:The water-soluble Polyether-containing Aminopolysiloxane (SPEAS)was synthesized, the viscosity, amino value and nd20 of which were 0.150~1.800 Pa•s, 0.200~0.596mmol/g and 1.6567~1.6685.The optimum conditions were 60~100℃(reaction temperature), 4~8 h (reaction time). Then the structures and properties of the samples were analyzed by FTIR,1H- NMR and TEM. Experimental results showed that the size of the particles of such aqueous dispersions at 2.0% are different. The bending rigidity of the treated fabric decreased (the soft hand-feeling enhanced), its wrinkle ecovery angle increased and static water absorption time downed to 1″48.

    • Film Morphology、Emulsification of Dodecyl/carboxyl Polysiloxane and Its Application Performance

      2010, 27(9).

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      Abstract:The film morphology of dodecyl/carboxyl modified polysiloxane (RCAS) on cotton fabric or the silicon wafer was investigated by field emission scanning electron microscope (FESEM) and atomic force microscope (AFM). The results showed that RCAS formed a relatively smooth film on the fabric surface. With the fabric terated by RCAS, the grooves on the fabric surface disappeared. What’s more, RCAS formed a micromorphology inhomogeneous and unsmooth film on the silicon wafer.There were many high or low bright peaks distributed at random on the film surface, especially as the field was 2×2μm2 and the date scale was 5nm in AFM observation. The application performance of RCAS emulsion and compounded emulsion on cotton fabric was also investigated.The application results indicated that RCAS emulsion and compounded emulsion provided the treated fabrics with good softness,compared to untreated fabric. Moreover, the bigger the concentration of RCAS emulsion in the compounded emulsion,the better the hydrophilicity and whiteness of the treated fabrics.Whereas the softness of the treated fabrics decreased.

    • >Oil field chemicals and petroleum additives
    • Study on the Interaction between Copolymer Acrylamide/2-acrylamido-2-methylpropanesulfonic acid/Octylacrylamide and Petroleum Sulfonate

      2010, 27(9).

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      Abstract:The viscosity, surface/interfacial activity and adsorption of copolymer acrylamide/2-acrylamido-2-methylpropanesulfonic acid/Octylacrylamide (HPPS) and petroleum sulfonate mixed system were studied. And the interaction was discussed. The results show that the viscosity of petroleum sulfonate/1.5g/L polymer HPPS mixed system increases as increasing the mass concentration of petroleum sulfonate, and reaches the maximum at mass concentration 2.0g/L, then viscosity declines fast. The surface tension of the mixed system is lower than that of single petroleum sulfonate when petroleum sulfonate mass concentration is below 0.5g/L, then the surface tension of the mixed system is higher than that of single petroleum sulfonate as the mass concentration increases. The interfacial tension between the mixed system and oil is higher than that of single petroleum sulfonate, but the minimum can reach 10-2mN/m. In polymer HPPS and 2.0g/L petroleum sulfonate mixed system the static adsorption of petroleum sulfonate on the reservoir sand increases as increasing the mass concentration of polymer HPPS, and reaches the maximum at HPPS mass concentration 3.0g/L.

    • >Acrylic series chemicals
    • Preparation of Perfluorinated acrylate Soap-free emulsion And Surface Properties of Membrane

      2010, 27(9).

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      Abstract:The Waterborne cationic perfluorinated acrylate soap-free emulsionwas prepared using perfluorinated alkyl ethyl acrylate (FM), methyl methacrylate (MMA), butyl acrylate (BA), octadecyl acrylate (ODA), methacryloxyethyl trimethylammonium chloride(DMC) as monomers, azobisisobutyronitrile (AIBN) as initiator and hydroxyl ethyl acrylate (HEA) as crosslinker. The structure of the copolymer was characterized in many ways. The contact angle of water and liquid paraffin on the fabric treated by the emulsion was 138癮nd 125皉espectively. The surface free energy of membrane was 19.01mJ/m2 when w(FM)=50%. The structure of fluorinated membrane surface appeared Lotus-Effect.

    • >Adhesives
    • Study of Modified Epoxy Curing Reagent by Oganosilicon and the Properties of Curing Product

      2010, 27(9).

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      Abstract:Novolac resin was modified by grafting reaction with condensation product of Polymethyl Triethoxy Silane and Polymethyltriethoxysilane, which could be used for curing epoxy resin. The different modified novolac resins were prepared from different ratio of materials and cured with epoxy resins. The cured products were tested by impact strength, glass transition temperature and thermogravimetric analysis. The results showed that the glass transition temperatures of modified cured products was 30℃ higher than the pure product, the impact strength increased more than 36.6%, and the thermal stability better.

    • >Building chemicals
    • Study on synthesis and properties of epoxy resin based on rosin

      2010, 27(9).

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      Abstract:Epoxy prepolymers were prepared via esterification reaction between acrylic acid rosin and 1,4-butanediol diglycidylether/1,6-hexanediol diglycidylether. Polyamide hardeners were synthesized via amidation reaction between acrylic acid rosin and diethylenetriamine/tetraethylenepentamine. Then a new series of polymers were obtained through the reaction between prepolymers and polyamide hardeners stoichiometrically. The tests showed the new polymers had moderate degree of hardness; cross cut test, less than 3; T-Bend, 0; impact resistance, more than 60kg•cm; chemical resistance, passed; and aging under ultraviolet lights for 30d, intact.

    • >Fine chemical intermediates
    • Hydroxyl protection - hydrosilylation method to prepare 1,3-bis(γ-hydroxypropyl)-1,1,3,3-tetramethyldisiloxane

      2010, 27(9).

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      Abstract:Tetraethoxysilane was reacted with allyl alcohol under the condition of sodium catalyst in ethanol, and the main product was triethoxyallyloxylsilane(I). I was reacted with 1,1,3,3-tetramethyldisiloxane in the presence of Platinum compound, and obtained 1,3-(γ-3-ethoxysiliconoxy-propyl)-1,1,3,3–tetramethyldisiloxane(II).1,3-bis(γ-hydroxypropyl)-1,1,3,3-tetramethyldisiloxane was received by homogeneous hydrolysiss of II in the mixed solvent of 2%Sodium hydroxide solution and ethanol. With the total yield of 76.4% in terms of 1,1,3,3-tetramethyldisiloxane. IR, HNMR, Gas chromatography / Mass spectrometry were used to characterize the intimidates and target product.

    • Synthesis of 2, 3-Benzosuberone

      2010, 27(9).

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      Abstract:2,3-benzosuberone was synthesized using benzene and glutaric anhydride as raw materials through Friedel-Crafts reaction, Wolff–Huang-Minlon reduction and cyclodehydration. Under the optimum reaction conditions of n(glutaric anhydride) :n(benzene):n(AlCl3)=1:2:2, at room temperature for 3h, and reduction at 120℃ for 2h, then cyclodehydration at 160℃ for 2h, the overall yield was 60.3%. Structures of the intermediates and the final product were characterized by IR, NMR and MS.

    • Acetylation of Phenols Catalysized by Solid Bases under solvent-free

      2010, 27(9).

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      Abstract:Supported solid base K2CO3/Al2O3 prepared under microwave irradiation were found to be an efficient catalyst for the acylation of phenols with acetic anhydride in high yields under solvent-free conditions and under microwave irradiation in a short reaction time. The catalysis efficacy of supported solid bases prepared under microwave irradiation, dipping and non-supported solid bases were investigated in the acylation of phenols with acetic anhydride at room temperature. It’s found that K2CO3/Al2O3 (III-3) prepared under microwave irradiation has the best catalysis in the solid bases in the reaction. Optimized the conditions of acetylation of phenol with K2CO3/Al2O3 (III-3), the experiment date shows that the best catalyst molar percent to phenol is 16.8mol% ,the best temperature is 60℃, the yield is 94.8% under these optimal conditions. K2CO3/Al2O3(III-3) as a efficient catalyst used in the acylation of various phenol donors was also investigated under microwave irradiation and traditional heating. The yields are 62.0%-99.8% under traditional heating in 150 min; 76.4%-100.0% under microwave irradiation in 9 min. The experimental data indicated that the general applicability and efficiency of this reaction is evident from the wide range of compounds studied. At the same time , microwave irradiation shorten reaction time largely , so it is better than the method of traditional heating.